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Catalyst and preparation method for preparing 4-aminodiphenylamine

A technology of aminodiphenylamine and nitrodiphenylamine, applied in the field of preparation of palladium/carbon catalysts, can solve the problems of no catalyst preparation method report, low activity, etc., and achieves reduction of uneven adsorption and aggregation, simple process, and reduction of recovery costs. Effect

Active Publication Date: 2019-03-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In summary, various patents have reported the application of nickel-based catalysts and palladium catalysts in the synthesis of RT-base. Different catalysts have large differences in selectivity and activity, and nickel-based catalysts generally have lower activity than noble metal catalysts. , but most of the patents have only reported the application of palladium / carbon catalyst in RT-base synthesis, and have not carried out detailed reports on the preparation method of the catalyst. Supported noble metal catalysts have good application prospects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The particle size is 0.25mm, the specific surface area is 800m 2 / g, activated carbon with ash content of 2%, soaked in a nitric acid solution with a mass fraction of 10%, boiled and refluxed for 10h, washed with distilled water to neutrality, after solid-liquid separation and water removal, added hydrogen peroxide with a mass fraction of 25% for 1h oxidation treatment , washed with distilled water to neutrality, solid-liquid separation and dehydration, and vacuum drying at 100°C for 4 hours to obtain a pretreated activated carbon carrier; add water to the pretreated activated carbon carrier and stir to form a carbon slurry, and chlorinated The palladium solution was continuously added to the carbon slurry within 30 minutes, stirred and impregnated for 8 hours; the sodium hypophosphite solution with a mass fraction of 20% was used to reduce for 4 hours; filtered, washed with distilled water until neutral; after solid-liquid separation and water removal, dry at 80°C for 1...

Embodiment 2

[0032] The particle size is 0.075mm, the specific surface area is 1500m 2 / g, activated carbon with ash content of 5%, soaked in a hydrochloric acid solution with a mass fraction of 30%, boiled and refluxed for 2h, washed with distilled water until neutral, after solid-liquid separation and water removal, added hydrogen peroxide with a mass fraction of 30% for oxidation treatment of 0.5 h, washed with distilled water to neutrality, solid-liquid separation and dehydration, and vacuum drying at 50°C for 16 hours to obtain a pretreated activated carbon carrier; add water to the pretreated activated carbon carrier and stir to form a carbon slurry, and add nitric acid with a mass fraction of 10% The palladium solution was continuously added to the carbon slurry within 5 minutes, stirred and impregnated for 2 hours; reduced with hydrazine hydrate solution with a mass fraction of 20% for 8 hours; filtered, washed with distilled water until neutral; after solid-liquid separation and wa...

Embodiment 3

[0035] The particle size is 0.15mm, the specific surface area is 1000m 2 / g, activated carbon with ash content of 4%, soaked in a nitric acid solution with a mass fraction of 50%, boiled and refluxed for 2h, washed with distilled water until neutral, after solid-liquid separation to remove water, add hydrogen peroxide with a mass fraction of 5% for 6h , washed with distilled water until neutral, after solid-liquid separation and dehydration, vacuum-dried at 80°C for 8 hours to obtain a pretreated activated carbon carrier; add water to the pretreated activated carbon carrier and stir to form a carbon slurry, and chlorinated The palladium solution was continuously added to the carbon slurry within 10 minutes, stirred and impregnated for 3 hours; the sodium hypophosphite solution with a mass fraction of 30% was used for reduction for 6 hours; filtered, washed with distilled water until neutral; after solid-liquid separation and water removal, dry at 50°C for 16 hours. Obtain the c...

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Abstract

The invention relates to a catalyst for preparing 4-aminodiphenylamine and a preparation method of the catalyst, and specifically provides a preparation method of a palladium / carbon catalyst for preparing the 4-aminodiphenylamine through hydrogenation. The catalyst is characterized in that activated carbon is used as a carrier, palladium is used as an active component, and a preparation process comprises the steps of pretreating the activated carbon, performing impregnation, performing reduction, performing washing, performing drying and the like. The prepared catalyst is used for a catalytic hydrogenation process of preparing the 4-aminodiphenylamine by a nitrobenzene method. Raw materials for preparing the catalyst disclosed by the invention are easy to obtain, the technology is simple, and the catalyst is used for preparing the 4-aminodiphenylamine through the hydrogenation, is high in activity and good in stability, and has good application prospects.

Description

technical field [0001] The invention relates to a catalyst and a preparation method for preparing 4-aminodiphenylamine, in particular to a preparation method of a palladium / carbon catalyst used for catalytic hydrogenation of nitrobenzene to synthesize 4-aminodiphenylamine. Background technique [0002] 4-aminodiphenylamine (commonly known as RT-base, also known as p-aminodiphenylamine) is an important organic intermediate, which is widely used in dyestuff, textile, printing, pharmaceutical and rubber additives industries. At present, it is mainly used in the rubber additive industry as an intermediate of p-phenylenediamine rubber anti-aging agent, and is the parent body of 40-type anti-aging agent (anti-aging agent 4010, 4010NA, 6PPD and 688, etc.) with excellent performance. [0003] There are more than 10 kinds of synthetic techniques for 4-aminodiphenylamine. At present, the production methods used for industrialization at home and abroad mainly include formanilide method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J35/10C07C211/55C07C209/36C07C209/38
Inventor 杨忠林金汉强李玉杰孙盛凯丁红霞
Owner CHINA PETROLEUM & CHEM CORP
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